# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 2114945'
loop_
_audit_author_name
_audit_author_address
'Ying Wang'
;College of Chemistry and Environmental Science, Hebei University
China
;
_audit_update_record             
;
2021-10-11 deposited with the CCDC.	2022-02-10 downloaded from the CCDC.
;
_audit_creation_date             2021-05-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(B2 O14 Pb12), 2(N0.5 O1.5)'
_chemical_formula_sum            'B N O10 Pb6'
_chemical_formula_weight         1427.96
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           59
_space_group_name_H-M_alt        'P m m n'
_space_group_name_Hall           '-P 2ab 2a'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z'
'-x-1/2, y, z'

_cell_length_a                   5.7481(5)
_cell_length_b                   9.4582(9)
_cell_length_c                   11.2770(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     613.09(10)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2775
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.37
_cell_measurement_theta_min      2.81
_shelx_estimated_absorpt_T_max   0.061
_shelx_estimated_absorpt_T_min   0.023
_exptl_absorpt_coefficient_mu    82.125
_exptl_absorpt_correction_T_max  0.0206
_exptl_absorpt_correction_T_min  0.0040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1705 before and 0.0827 after correction. The Ratio of minimum to maximum transmission is 0.1942. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    7.735
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.134
_exptl_crystal_size_min          0.077
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6656
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.530
_diffrn_reflns_theta_min         2.811
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                696
_reflns_number_total             823
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.926
_refine_diff_density_min         -1.843
_refine_diff_density_rms         0.440
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         823
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0327
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0561P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0918
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.750000 0.55607(7) 0.82033(7) 0.0357(2) Uani 1 2 d S T P . .
Pb2 Pb 0.250000 0.250000 0.86576(10) 0.0363(3) Uani 1 4 d S T P . .
Pb3 Pb 0.750000 0.250000 0.64357(10) 0.0347(3) Uani 1 4 d S T P . .
Pb4 Pb 0.250000 0.01269(8) 0.61924(6) 0.0359(2) Uani 1 2 d S T P . .
N1 N 0.250000 0.750000 0.914(3) 0.054(7) Uani 1 4 d S T P . .
B1 B 0.750000 0.750000 0.569(3) 0.039(7) Uani 1 4 d S T P . .
O1 O 0.250000 0.639(2) 0.963(2) 0.100(7) Uani 1 2 d S T P . .
O2 O 0.250000 0.750000 0.800(2) 0.080(9) Uani 1 4 d S T P . .
O3 O 1.0015(14) 0.3972(8) 0.7542(7) 0.0325(19) Uani 1 1 d . . . . .
O4 O 0.750000 0.6199(15) 0.6294(14) 0.053(4) Uani 1 2 d S T P . .
O5 O 0.250000 0.250000 0.5512(17) 0.037(4) Uani 1 4 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Pb1 3.6684(14) 2_665 ?
Pb1 O3 2.215(8) . ?
Pb1 O3 2.215(8) 8_755 ?
Pb1 O4 2.236(15) . ?
Pb2 Pb4 3.5730(11) 2 ?
Pb2 Pb4 3.5730(11) . ?
Pb2 O3 2.358(8) 1_455 ?
Pb2 O3 2.358(8) 8_755 ?
Pb2 O3 2.358(8) 2_655 ?
Pb2 O3 2.358(8) 7_465 ?
Pb3 Pb4 3.6570(5) 2_655 ?
Pb3 Pb4 3.6569(5) . ?
Pb3 Pb4 3.6570(5) 2 ?
Pb3 Pb4 3.6570(5) 1_655 ?
Pb3 O3 2.363(8) 7_565 ?
Pb3 O3 2.363(8) . ?
Pb3 O3 2.363(8) 2_655 ?
Pb3 O3 2.363(8) 8_755 ?
Pb4 O3 2.254(8) 2_655 ?
Pb4 O3 2.254(8) 7_465 ?
Pb4 O5 2.372(6) . ?
N1 O1 1.19(3) . ?
N1 O1 1.19(3) 2_565 ?
N1 O2 1.28(4) . ?
B1 O4 1.41(2) 2_665 ?
B1 O4 1.41(2) . ?
B1 O5 1.35(4) 5_666 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Pb1 Pb1 132.7(2) . 2_665 ?
O3 Pb1 Pb1 132.7(2) 8_755 2_665 ?
O3 Pb1 O3 81.5(4) . 8_755 ?
O3 Pb1 O4 81.9(3) . . ?
O3 Pb1 O4 81.9(4) 8_755 . ?
O4 Pb1 Pb1 74.3(4) . 2_665 ?
Pb4 Pb2 Pb4 77.83(3) . 2 ?
O3 Pb2 Pb4 87.45(19) 8_755 . ?
O3 Pb2 Pb4 38.19(19) 1_455 2 ?
O3 Pb2 Pb4 38.19(19) 8_755 2 ?
O3 Pb2 Pb4 87.45(19) 1_455 . ?
O3 Pb2 Pb4 87.45(19) 2_655 2 ?
O3 Pb2 Pb4 38.19(19) 2_655 . ?
O3 Pb2 Pb4 38.19(19) 7_465 . ?
O3 Pb2 Pb4 87.45(19) 7_465 2 ?
O3 Pb2 O3 74.6(4) 7_465 2_655 ?
O3 Pb2 O3 74.6(4) 8_755 1_455 ?
O3 Pb2 O3 115.5(4) 7_465 8_755 ?
O3 Pb2 O3 72.3(4) 8_755 2_655 ?
O3 Pb2 O3 115.5(4) 1_455 2_655 ?
O3 Pb2 O3 72.3(4) 7_465 1_455 ?
Pb1 Pb3 Pb4 123.23(2) 2_655 2 ?
Pb1 Pb3 Pb4 62.422(13) 2_655 . ?
Pb1 Pb3 Pb4 123.23(2) 2_655 2_655 ?
Pb1 Pb3 Pb4 62.421(13) 2_655 1_655 ?
Pb4 Pb3 Pb4 171.39(4) . 2_655 ?
Pb4 Pb3 Pb4 75.72(2) 2_655 1_655 ?
Pb4 Pb3 Pb4 103.611(19) . 1_655 ?
Pb4 Pb3 Pb4 75.724(19) . 2 ?
Pb4 Pb3 Pb4 103.61(2) 2_655 2 ?
Pb4 Pb3 Pb4 171.39(4) 1_655 2 ?
O3 Pb3 Pb1 38.32(19) 2_655 2_655 ?
O3 Pb3 Pb1 100.71(19) 8_755 2_655 ?
O3 Pb3 Pb1 38.32(19) 7_565 2_655 ?
O3 Pb3 Pb1 100.71(19) . 2_655 ?
O3 Pb3 Pb4 151.89(19) 2_655 2_655 ?
O3 Pb3 Pb4 36.60(19) 2_655 . ?
O3 Pb3 Pb4 85.43(19) 7_565 2_655 ?
O3 Pb3 Pb4 36.60(19) . 2_655 ?
O3 Pb3 Pb4 85.43(19) 2_655 2 ?
O3 Pb3 Pb4 36.60(19) 8_755 2 ?
O3 Pb3 Pb4 99.14(19) . 2 ?
O3 Pb3 Pb4 99.15(19) 7_565 . ?
O3 Pb3 Pb4 151.89(19) 7_565 2 ?
O3 Pb3 Pb4 36.60(19) 7_565 1_655 ?
O3 Pb3 Pb4 85.43(19) . 1_655 ?
O3 Pb3 Pb4 151.89(19) 8_755 1_655 ?
O3 Pb3 Pb4 85.43(19) 8_755 . ?
O3 Pb3 Pb4 99.14(19) 2_655 1_655 ?
O3 Pb3 Pb4 151.89(19) . . ?
O3 Pb3 Pb4 99.14(19) 8_755 2_655 ?
O3 Pb3 O3 75.5(4) 2_655 7_565 ?
O3 Pb3 O3 72.2(4) . 7_565 ?
O3 Pb3 O3 116.3(4) . 2_655 ?
O3 Pb3 O3 75.5(4) . 8_755 ?
O3 Pb3 O3 72.2(4) 2_655 8_755 ?
O3 Pb3 O3 116.3(4) 7_565 8_755 ?
Pb2 Pb4 Pb3 63.645(19) . 1_455 ?
Pb2 Pb4 Pb3 63.645(19) . . ?
Pb3 Pb4 Pb3 103.61(2) . 1_455 ?
O3 Pb4 Pb2 40.3(2) 7_465 . ?
O3 Pb4 Pb2 40.3(2) 2_655 . ?
O3 Pb4 Pb3 38.67(19) 7_465 1_455 ?
O3 Pb4 Pb3 102.4(2) 2_655 1_455 ?
O3 Pb4 Pb3 38.67(19) 2_655 . ?
O3 Pb4 Pb3 102.4(2) 7_465 . ?
O3 Pb4 O3 78.6(4) 2_655 7_465 ?
O3 Pb4 O5 82.0(4) 7_465 . ?
O3 Pb4 O5 82.0(4) 2_655 . ?
O5 Pb4 Pb2 70.0(4) . . ?
O5 Pb4 Pb3 56.19(14) . . ?
O5 Pb4 Pb3 56.19(14) . 1_455 ?
O1 N1 O1 124(4) . 2_565 ?
O1 N1 O2 118.1(19) 2_565 . ?
O1 N1 O2 118.1(19) . . ?
O4 B1 O4 122(3) 2_665 . ?
O5 B1 O4 119.1(13) 5_666 2_665 ?
O5 B1 O4 119.1(13) 5_666 . ?
Pb1 O3 Pb2 128.0(3) . 1_655 ?
Pb1 O3 Pb3 100.3(3) . . ?
Pb1 O3 Pb4 112.6(3) . 2_655 ?
Pb2 O3 Pb3 107.7(3) 1_655 . ?
Pb4 O3 Pb2 101.5(3) 2_655 1_655 ?
Pb4 O3 Pb3 104.7(3) 2_655 . ?
B1 O4 Pb1 134.8(16) . . ?
Pb4 O5 Pb4 142.2(9) . 2 ?
B1 O5 Pb4 108.9(4) 5_666 2 ?
B1 O5 Pb4 108.9(4) 5_666 . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_ww
_database_code_depnum_ccdc_archive 'CCDC 2114946'
loop_
_audit_author_name
_audit_author_address
'Ying Wang'
;College of Chemistry and Environmental Science, Hebei University
China
;
_audit_update_record             
;
2021-10-11 deposited with the CCDC.	2022-02-10 downloaded from the CCDC.
;
_audit_creation_date             2021-05-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(B4 F2 N2 O22 Pb12)'
_chemical_formula_sum            'B2 F N O11 Pb6'
_chemical_formula_weight         1473.77
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   6.8025(7)
_cell_length_b                   11.5092(9)
_cell_length_c                   8.8989(9)
_cell_angle_alpha                90
_cell_angle_beta                 101.704(4)
_cell_angle_gamma                90
_cell_volume                     682.22(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8596
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.53
_shelx_estimated_absorpt_T_max   0.156
_shelx_estimated_absorpt_T_min   0.022
_exptl_absorpt_coefficient_mu    73.830
_exptl_absorpt_correction_T_max  0.0481
_exptl_absorpt_correction_T_min  0.0007
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1015 before and 0.0698 after correction. The Ratio of minimum to maximum transmission is 0.0146. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    7.174
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            19582
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         2.337
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1462
_reflns_number_total             1645
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         1.811
_refine_diff_density_min         -1.526
_refine_diff_density_rms         0.340
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     106
_refine_ls_number_reflns         1645
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0231
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0298P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0570
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.05853(5) 0.250000 0.41655(5) 0.02671(12) Uani 1 2 d S T P . .
Pb2 Pb 0.43538(4) 0.09341(2) 0.20468(4) 0.02752(10) Uani 1 1 d . . . . .
Pb3 Pb 0.60626(6) 0.250000 0.59530(5) 0.02739(12) Uani 1 2 d S T P . .
Pb4 Pb 1.08949(4) 0.40691(2) 0.79735(4) 0.02779(10) Uani 1 1 d . . . . .
N1 N 0.7494(15) 0.250000 0.0105(13) 0.040(3) Uani 1 2 d S T P . .
B1 B 0.7455(11) -0.0015(8) 0.5038(12) 0.030(2) Uani 1 1 d . . . . .
F1 F 1.2805(15) 0.250000 0.9568(14) 0.079(3) Uani 1 2 d S T P . .
O1 O 0.7622(14) 0.3449(6) -0.0549(10) 0.067(2) Uani 1 1 d . . . . .
O2 O 0.7154(13) 0.250000 0.1454(11) 0.044(2) Uani 1 2 d S TU P . .
O3 O 0.6752(9) 0.0992(4) 0.4301(7) 0.0331(13) Uani 1 1 d . . . . .
O4 O 0.7729(9) -0.0991(4) 0.4226(7) 0.0322(13) Uani 1 1 d . . . . .
O5 O 0.7925(8) -0.0026(5) 0.6634(7) 0.0368(14) Uani 1 1 d . . . . .
O6 O 0.3545(11) 0.250000 0.3113(10) 0.0305(18) Uani 1 2 d S T P . .
O7 O 0.9586(10) 0.250000 0.6800(9) 0.0243(15) Uani 1 2 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O4 2.390(6) 3_656 ?
Pb1 O4 2.390(6) 2_656 ?
Pb1 O6 2.387(7) . ?
Pb1 O7 2.570(8) 1_455 ?
Pb2 Pb2 3.6046(6) 4_565 ?
Pb2 O2 2.750(7) . ?
Pb2 O3 2.316(6) . ?
Pb2 O5 2.369(5) 3_656 ?
Pb2 O6 2.159(4) . ?
Pb3 O3 2.381(6) . ?
Pb3 O3 2.381(6) 4_565 ?
Pb3 O6 2.751(9) . ?
Pb3 O7 2.362(7) . ?
Pb4 Pb4 3.6118(6) 4_565 ?
Pb4 F1 2.493(6) . ?
Pb4 O4 2.336(6) 2_756 ?
Pb4 O5 2.395(6) 4_565 ?
Pb4 O7 2.184(4) . ?
N1 O1 1.249(9) . ?
N1 O1 1.249(9) 4_565 ?
N1 O2 1.267(14) . ?
B1 O3 1.369(11) . ?
B1 O4 1.369(11) . ?
B1 O5 1.392(12) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Pb1 O4 93.2(3) 2_656 3_656 ?
O4 Pb1 O7 68.74(17) 3_656 1_455 ?
O4 Pb1 O7 68.74(17) 2_656 1_455 ?
O6 Pb1 O4 84.0(2) . 2_656 ?
O6 Pb1 O4 84.0(2) . 3_656 ?
O6 Pb1 O7 139.3(3) . 1_455 ?
O2 Pb2 Pb2 49.05(12) . 4_565 ?
O3 Pb2 Pb2 88.34(13) . 4_565 ?
O3 Pb2 O2 75.7(2) . . ?
O3 Pb2 O5 90.0(2) . 3_656 ?
O5 Pb2 Pb2 116.18(15) 3_656 4_565 ?
O5 Pb2 O2 158.8(2) 3_656 . ?
O6 Pb2 Pb2 33.42(17) . 4_565 ?
O6 Pb2 O2 77.6(2) . . ?
O6 Pb2 O3 78.0(3) . . ?
O6 Pb2 O5 84.3(2) . 3_656 ?
O3 Pb3 O3 93.6(3) . 4_565 ?
O3 Pb3 O6 66.21(17) . . ?
O3 Pb3 O6 66.21(17) 4_565 . ?
O7 Pb3 O3 83.27(19) . . ?
O7 Pb3 O3 83.27(19) . 4_565 ?
O7 Pb3 O6 134.1(2) . . ?
F1 Pb4 Pb4 43.58(16) . 4_565 ?
O4 Pb4 Pb4 88.31(12) 2_756 4_565 ?
O4 Pb4 F1 101.8(3) 2_756 . ?
O4 Pb4 O5 92.2(2) 2_756 4_565 ?
O5 Pb4 Pb4 117.37(15) 4_565 4_565 ?
O5 Pb4 F1 154.9(3) 4_565 . ?
O7 Pb4 Pb4 34.20(16) . 4_565 ?
O7 Pb4 F1 77.8(2) . . ?
O7 Pb4 O4 76.6(2) . 2_756 ?
O7 Pb4 O5 85.5(2) . 4_565 ?
O1 N1 O1 122.0(12) 4_565 . ?
O1 N1 O2 119.0(6) 4_565 . ?
O1 N1 O2 119.0(6) . . ?
O3 B1 O5 118.8(8) . . ?
O4 B1 O3 120.9(8) . . ?
O4 B1 O5 120.2(8) . . ?
Pb4 F1 Pb4 92.8(3) 4_565 . ?
Pb2 O2 Pb2 81.9(2) . 4_565 ?
N1 O2 Pb2 116.6(5) . 4_565 ?
N1 O2 Pb2 116.6(5) . . ?
Pb2 O3 Pb3 111.3(2) . . ?
B1 O3 Pb2 120.4(5) . . ?
B1 O3 Pb3 114.5(6) . . ?
Pb4 O4 Pb1 107.3(2) 2_746 3_656 ?
B1 O4 Pb1 112.4(6) . 3_656 ?
B1 O4 Pb4 122.6(5) . 2_746 ?
Pb2 O5 Pb4 121.8(3) 3_656 4_565 ?
B1 O5 Pb2 118.2(5) . 3_656 ?
B1 O5 Pb4 120.0(5) . 4_565 ?
Pb1 O6 Pb3 93.3(3) . . ?
Pb2 O6 Pb1 118.87(17) . . ?
Pb2 O6 Pb1 118.87(17) 4_565 . ?
Pb2 O6 Pb2 113.2(3) . 4_565 ?
Pb2 O6 Pb3 103.7(2) . . ?
Pb2 O6 Pb3 103.7(2) 4_565 . ?
Pb3 O7 Pb1 98.5(3) . 1_655 ?
Pb4 O7 Pb1 106.2(2) 4_565 1_655 ?
Pb4 O7 Pb1 106.2(2) . 1_655 ?
Pb4 O7 Pb3 116.20(19) . . ?
Pb4 O7 Pb3 116.20(19) 4_565 . ?
Pb4 O7 Pb4 111.6(3) 4_565 . ?

_olex2_submission_special_instructions 'No special instructions were received'
